Posts by sumorga

Application of Alkylbenzoic Acid Intermediates

Application of alkylbenzoic acid intermediates: Alkylbenzoic acid is a very important organic chemical intermediate, with wide use in preservatives, protection agents, pesticides, pharmaceuticals, organic dyes, photographic materials, disinfectant, fluorine-containing pharmaceutical and other fields.

Alkylbenzoic acid is a raw material of synthesizing alkylcyclohexyl carboxylic acid, alky carboxylate, fluorinated benzoic acid and other organic chemical products. Besides, it is popular in ester liquid crystals.

Recently, studies on alkylbenzoic acid intermediates have been booming. A series of alkylbenzoic acid products have been developed. They mainly are: Methyl benzoate, ethyl benzoate, isopropyl benzoate, p-tert-butyl benzoic acid,etc. P-tert-butyl benzoic acid (PTBBA), also named para-tert-butyl benzoic acid, 4-tert-butylbenzoate, 4-(tert-butyl) benzoic acid, etc, is colorless needle crystalline or crystal powder. It is a very important intermediate for organic synthesis and the main usages are: modifier of alkyd resin; additive of cutting oil and lubricating oil; nucleating agent of polypropylene; food preservatives; Polyester polymerization moderator; additives of car deodorizer, outer membrane of oral drug, alloy preservatives, lubricity additives, polypropylene nucleating agent, heat stabilizer for PVC, metal processing cutting fluid, antioxidant, alkyd resin improving agent, flux, dyes and novel sunscreen agent; it is also used for production of methyl p-tert-butyl benzoate, which is widely used in chemical synthesis, cosmetics, flavors and fragrances and other industries. Its barium, sodium, zinc salts could be used as stabilizer of polyethylene.

Synthesis methods of P-tert-butyl benzoic acid.

(1)Solvent-free liquid phase oxidation method

(2)Nitric acid oxidation method

(3)Acetate solvent catalytic oxidation method

(4)Microwave radiation method

(5)Potassium permanganate oxidation method

The solvent-free liquid phase oxidation method

This method takes p-tert-butyl toluene (PTBT) as the raw material, Cobalt acetate as catalyst. Using 40% acetaldehyde as initiator agent will shorten the induction period. The reaction is at a temperature of 170 ℃. After 100 min, the p-tert-butyl benzoic acid productivity is 50%, with selectivity of 98%. It is ensured that the reaction has turned to be first degree at 170 ℃, the oxidation reaction rate just have connect with the concentration of PTBT. The procedures are: the oxidation reaction device is 2L autoclave, with speed adjustable stirrer. The autoclave bottom is an air distribution. The top is connected with condenser. PTBT after condensation and yielded water pour into the separation tank. The upper layer PTBT go back to the autoclave and underlayer water is taken out. Exhaust gas exit is connected with oxygen analyzer, to test the oxygen consumption in the reaction and judge the progress of the reaction. Sampling in a certain period to test p-tert-butyl toluene content in the reaction solution and analyzing the relationship of yielded p-tert-butyl benzoic acid quantity with reaction.

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Preparation of P-toluenesulfonic Acid

The purpose of the experiment:

To learn preparation of aryl sulfonic acid with aromatic sulfonation reaction;

To consolidate the use, reflus and recrystallization opearation of water knockout trap.

 

The principle of the reaction:

The main reaction:

The vise reaction:

Steps:

Reflux reaction: adding 25 mL Toluene into the 50 mL round-bottom flask first. Then adding 5.5 ml concentrated sulfuric acid slowly, while the flask is being shaken. At last, throwing several grains of zeolite into the flask. Heating and refluxing the flask on asbestos network for 2h till the volume of liquid in the water knockout trap to be 2 mL.

Equipments:

a Reaction device b Filtration device

Product separation: keep the reactants to be cool. Put the reactants into 60 mL erlenmey flask. Adding 1.5 mL water till there is some crystal coming out. Stirring the reactants slowly with glass rod. When the reactants become solid, filtering the reactants with Buchner funnel. Pressing the reactants to remove Toluene and p-toluenesulfonic acid and getting crude product 15g. Purification: To get pure p-toluenesulfonic acid (PTSA http://www.p-toluenesulfonicacid-ptbba.com ), the crude product should be recrystallized. Dissolving 12g crude product with 6 mL water in 50mL beaker ( or large test tube). Passing hydrogen chloride gas into the solution till there is some crystal coming out. When the hydrogen chloride gas is being ventilated, some measures should be taken to avoid “suck down”. Sucting and filtering the precipitated crystals with Buchner funnel rapidly and then wash the rest crystals with small amount of concentrated hydrochloride acid. After squeezing the water out with glass stopper, store the solid in dryer.

Notice:

While the concentrated sulfonic acid was dropped in, the flask must be shaken and the dropping rate should be slow with burette.

The heating strength should be under control.

Stirring when the crystals come out.

Packing of P-Toluenesulfonic Acid (PTSA):

Pharmaceutical, industrial and refined grades P-Toluenesulfonic Acid (PTSA) are packed in plastic woven bag with film inner, net weight is 25kg. Reagent grade product is packed in paper fiber drums with film inner as well. The net weight is 35kg. Of course, we would make package as per customers’ request.

Notice of operating P-Toluenesulfonic Acid (PTSA):

The operating staff should pass the professional train and operate P-Toluenesulfonic Acid (PTSA) according to the working rules strictly. The operating staff is proposed to wear a dust mask, jumpsuit rubber protective clothing and gloves. The package should be far away from fire, heat source. No smoking at the working place. Explosion proof ventilation systems and equipment are used, avoiding dust and contact with oxidizing agents, alkalis. When loading and unloading, it should be light, to prevent the package and container from being damaged.

Notice of storing P-Toluenesulfonic Acid (PTSA):

P-Toluenesulfonic Acid (PTSA) should be stored in a cool, ventilated warehouse, and separated with food chemicals, avoiding mixing reservoir. The warehouse should be equipped with the appropriate variety and quantity of fire equipment, emergency equipment and suitable host material spill. Empty containers may be harmful residues.

Transportation Notice of P-Toluenesulfonic Acid (PTSA):

Starting the shipment should make sure the package is closed and loading should be safe. To ensure the container does not leak, fall, drop, damage on the way. Strictly forbid mixed loading or mixed transportation with oxidizing agents, alkalis and food chemicals. Transit should be anti-exposure, anti-rain and anti-high temperature. Transport travel must be cleaned thoroughly, disinfected. Otherwise, it is not allow to ship other items.

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Synthesis of P-Tert-Butyl Benzoic Acid

Abstract: P-tert-butyl toluene PTBT as the raw material, Oxygen as the oxidant, Glacial Acetate acid as the solvent, and Cobalt acetate as the catalyst. Studying the factors influencing P-tert-butyl benzoic acid (PTBBA) synthesis and fixing the best conditions for this process occurred on: the temperature is 90-95℃,the ratio between raw material and solvent is 1:4(m:m), the concentrate of catalyst is w=0.1-0.2, P-tert-butyl toluene(PTBT)’s conversion rate could up to 100% and the yield is 87%.

Key wards: P-tert-butyl toluene(PTBT) P-Tert-Butyl Benzoic Acid(PTBBA) Oxidization Synthesize

P-Tert-Butyl Benzoic Acid(PTBBA) is colorless needle crystal or crystalline powder, derivative of benzoic acid, and a important organic synthesis intermediate. Its main purposes are: (1) Used as modifier for alkyd resin production; (2) Used as additives for cutting oils and lubricants; (3) Used as nucleating agent of polypropylene; (4) Its barium, sodium, zinc salts could be used as stabilizer of polyvinyl chloride; (5) Used as food additives; (6) Used as regulator for polyester polymerization reaction and so on.

In 1930s, this product in laboratory research begun. Currently, there are product launching in America, Japan, Germany and other countries markets. However, our domestic production was not well developed, making home consumption of this product, especially the polyvinyl chloride and polypropylene industry, rely on import. Therefore, study and development on P-Tert-Butyl Benzoic Acid(PTBBA) has broad prospects.

Nitric acid oxidation method

Preparation of crude PTBBA: Adding 26mL (0.2mol,29.6g) p-tert-butyl toluene (PTBT), 26mL 68%(0.4mol,37g) Nitric acid, and then 215mL water into the 500 mL autoclave. Closing the lid and starting the stirrer. The temperature is heated to 180℃ and the traction time is kept to be 8 h. After water cooling off, the cover was removed. Majority of the solids deposited at the autoclave bottom, and some was attaching to the cooling pipes. Collecting the solid, filtrating and drying, the weight is 34.5 g and productivity is 95.5%.

Purifying P-tert-butyl benzoic acid: Weighting 10g Sodium Hydroxide and making it into 10% solution with 90 mL water. Adding above solid into the solution. After completely dissolved, filtrating it. Adjusting the filtrate’s ph value to be around 3 with Hydrochloric acid. Then there is large quantity of crystalline happening. Stewing and filtrating, 33.4g material will be yielded and the productivity is 98.2%.

Even if the productivity is high with Nitric acid oxidation method to prepare P-tert-butyl benzoic acid, the causticity of nitric acid to the devices is great. During the reaction, the side products, such as nitrogen oxides, have great effect on the environment.

Acetate solvent catalytic oxidation method:

This method takes p-tert-butyl toluene (PTBT) as raw material, Cobalt Acetate as the catalyst and acetate acid as solvent. 250 mL stainless steel autoclave is the main reaction device, with mechanical stirrer. The air inlet and products outlet are at the bottom of the autoclave. The reaction is free redical chain reaction. The theory is below:

High temperature make p-tert-butyl toluene (PTBT) oxidized to yield P-tert-butyl benzoic acid with suitable catalyst. The productivity is high, but there is too many side products and the reaction takes too long time.

Microwave Radiation Method: The procedures are: adding 6 mL p-tert-butyl toluene, 8.4g Potassium Permanganate, 1.0g Benzyl triethyl ammonium chloride and 100mL water into 250 mL three-necked flash one by one. Shaking up and put it into the microwave reactor, assembling motor stirrer, reflux condenser and thermograph. Adjusting the microwave radiation power at 660W and keeping radiating for 50 min. After the reaction finished, pumping and filtering away Manganese Dioxide and get the remained solution concentrated and cooled to room temperature. Adding Hydrochloric acid to adjust the PH to be 2-3, cooling the solution till there is some crystalline come out. That is crude P-tert-butyl Benzoic acid (PTBBA). The fined products should be recrystallized with Toluene, the weight is 5.6g. And it is white needle crystalline. The final productivity is 82.6%. Melting point is 164-166℃.

Potassium Permanganate Oxidation Method:

The procedures are: adding Toluene dried by Calcium Chloride anhydrous, and 30g Aluminium Trichloride powder into the 250mL three-necked flash with reflux condenser and motor stirrer. Splashing 40g dried tert-butyl alcohol into the flash slowly. Transferring the solution into 500 mL beaker and adding about 200g crushed ice. Layering and washing it with salt solution. Reducing the press and remove the remained Toluene.

Adding 300mL deionized water and 54.5g p-tert-butyl toluene into the 500mL three-necked flash, which is connected with reflux condenser and motor stirrer. While heating and stirring rapidly, adding Potassium Permanganate in lots. Keeping the reaction conducting 7-8 h till the purple solution doesn’t fade. Putting the solution into 500mL beaker and keeping it for one night. After filtering Manganese Dioxide away , adding hydrochloric acid. Repeating above procedures till the color turns into colorless and PH valued gets to be below 5. After washing, adding 100mL toluene white solid to be dissolved. The upper layer was reduced press to recover toluene. Cooling to obtain needle crystalline P-Tert-Butyl Benzoic Acid(PTBBA).

In the series reports of studies on synthesizing P-tert-butyl Benzoic acid (PTBBA), the methods, such as Microwave Radiation Method, Potassium Permanganate Oxidation Method, Nitric acid oxidation method, Acetate solvent catalytic oxidation method and the Solvent-free liquid phase oxidation method, have been introduced in details. Besides, there some other methods, like high-temperature gas-phase oxidation method. While being catalyzed, p-tert-butyl toluene is gasified and oxidized by the high temperature and yield Para-tert-butyl Benzoic acid (PTBBA). The electronic oxidization method is also workable in P-tert-butyl Benzoic acid’s preparation.

Application and Development Prospects of P-tert-butyl Benzoic acid (PTBBA): Sunscreens is the core of sunscreen cosmetics formulations. In 1928, USA released the first report on sunscreens all over the world. Till now, there are already forty kinds of sunscreens being developed. According to the function, they are divided into UV absorbers and Ultraviolet bulk toners. In 1997, Pursol 1789 was approved by USA FDI as safe and effective sunscreen. It is the most effective one among the rare kinds of UVA type absorbers. The structure is below:

With the wide use of polyvinyl chloride (PVC) in industry, agriculture, health care, daily necessities and other fields, the PVA heat stabilizer P-tert-butyl Benzoic acid (PTBBA)’s consumption is rising year by year. At present, many domestic PVC stabilizer producers are using P-tert-butyl Benzoic acid, mainly the liquid type. Korea, Japan, Mexico, Europe, America, India, Netherlands and other countries’ firms are also using it with large quantity. In addition, the market demand as lubricants adhesives and dye auxiliaries is also getting larger. Currently, America, Japan, Germany and other countries have developed P-tert-butyl Benzoic acid (PTBBA) production technique and have products available for the market. In the international market, only the France and Japan’s output has reached 18000 tons. However, our country’s export was only 300 ton last year. It is obvious that this product not only has large share for export, but the domestic demand is large. From the domestic and international market demand, the P-tert-butyl Benzoic acid (PTBBA) still has a huge shortfall in supply. So far, the P-tert-butyl Benzoic acid process synthetic route is not perfect , efficient , energy-saving , environmentally – friendly production process still has a practical application of the value .

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Sodium p-toluenesulfonate

Sodium p-toluenesulfonate is a white powdery, dihydrous crystalline substance that is easily soluble in water. Usually by toluene sulfonation using alkali neutralization after made: by toluene as raw material, through sulfonation of methyl benzene sulfonic acid and reoccupy raw made by liquid alkali neutralization, decoloring, concentration and crystallization, centrifugal to finished products.
Sodium p-toluenesulfonate is mainly used as the adjuvant of synthetic detergents, auxiliary solvents, and pharmaceutical intermediates. Sizing adjuvant for chemical industry and synthetic detergents; As a water aid solvent for synthetic detergents, water content can be increased when mixed with powdery detergents. It is also used as a crystalline additive in fertilizer production. In liquid detergent, it is mainly used to increase solvents. When sodium p-toluene sulfonate is added, the viscosity and turbidity will decrease. When used, attention should be paid to the content of raw materials, inorganic salt and solubility. Especially for liquid detergent, its salt content has a great influence on liquid transparency. Used in the organic synthesis industry, in medicine for the synthesis of doxycycline, pansperidine, naproxen and for the production of amoxicillin and cephalosporin intermediates.
If you have the demand for this product, please contact us – Nanjing Jianci Chemical Plant Co.,Ltd.

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How to prepare benzene sulfonic-acid?

Benzene sulfonic-acid is a colorless needle or flake crystal, which easy to dissolve in water and ethanol, but insoluble in ether and carbon disulfide.
Using benzene as raw materials,after liquid trioxide sulfonation and its chemical equations as follows: PhH+HO-SO3H—-△→PhSO3H+H2O. Adding 93% sulphur trioxide 2400 l sulfonated pot, the benzene in the velocity of 2500-3000 l/h flow into the evaporator, after evaporation and overheating temperature of 150 ℃ above the overheating of benzene vapor, through bubbler in sulfate layer reaction, temperature about 170 ℃, the last free acid control in 4-5%. The reaction was completed around 10h, and the unreacted benzene vapor and the generated water vapor were separated by condensation, and the acid benzene was recycled by the liquid alkali neutralization and salt dehydration. Benzene sulfonic acid with benzene sulfonic acid and benzene sulfonic acid. The consumption of raw materials in the preparation process is: 600 tons of benzene per kg, and 750 tons of sulphuric acid per kilogram.
If you are interested in preparing benzene sulfonic-acid, you can call us – Nanjing Jianci Chemical Plant Co.,Ltd.

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Cosolvent sodium xylene sulphonate

Sodium Xylene Sulphonate is a new type of high efficient low toxicity of washing supplies solubilization conditioners. It is used as detergent additives and solubilizer in detergent, which is also used as a component dry cleaners, fungicide and metal processing cleansing agents, etc. Sodium xylene sulphonate is used in liquid detergent, which can be used as water soluble aid and reduce the turbidity point and viscosity.
Surfactant refers to a substance with a fixed hydrophilic group, which can be aligned on the surface of the solution and can cause a significant decrease in surface tension.Sodium xylene sulphonate is not a real surfactant, but it is a cosolvent.It can have a good solubilization and reduced viscosity effect on the surfactant.
Compared with products that use traditional solvent, the washing products using sodium xylene sulphonate have better feeling, lower irritation and higher purity.If you want to buy it, you can come to our company – Nanjing Jianci Chemical Plant Co.,Ltd.

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The General Analysis of Sodium Xylene Sulphonate

Sodium Xylene Sulphonate SXS is an effective hydrotrope for water solutions of various surfactants and hydrophylic solvents. Due to Sodium Xylene Sulfonate’s dissolving abilities, SXS is often added to shampoos as a thickening agent that helps suspend other ingredients.
Since Sodium Xylene Sulphonate has no detergency, Amphoteric or Phosphate Ester surfactants which contribute both detergency and hydrotroping power to the cleaner are used in high performance formulations.
Sodium Xylene Sulfonate is considered a low hazard ingredient by the Cosmetics Database, which has mild concerns regarding organ system toxicity and skin and eye irritation. It is FDA approved, and is seen in shampoos and other products in concentrations up to 10%.
Nanjing Jianci Chemical Plant Co.,Ltd found in 1990, is located in Jiangbei Industry Zone of Nanjing, Jiangsu Province, which is near the beautiful Yangtze River. Our plant covers an area of 50,000 square meters with the registered capital of RMB 100 million.
Our products mainly involve two series: series of ParaToluenesulfonic Acid and ParaTertButyl Benzoic Acid. Series of 4-Toluene Aulfonic Acid: P-Toluenesulfonic Acid PTSA, P -Toluene Sulfonic Acid 65% water solution, Sodium P-Toluene Sulfonate, Sodium Xylene Sulphonate and its main raw materials.

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Production of P-Tert-Butyltoluene(4-tert-Butyltoluene)

p-tert-Butyl Toluene(C11H16) is used as a solvent for resins which is used as an intermediate for organic synthesis, especially for tert-Butylbenzoic Acid, used as a fixative of fragrance.
It is well-known that P-Tert-Butyltoluene is also known as 4-tert-Butyltoluene which is clear colorless liquid with an aromatic gasoline-like odor. It may react with oxidizing materials.
The Preparation of 4-tert-Butyltoluene is putting toluene placed in a reactor, and adding catalyst, tert butyl chloride, reaction after the washing layered, organic distilled products. You can also use different butene alkylation of toluene in the presence of sulfuric acid and product creation.
Nanjing Jianci Chemical Plant Co.,Ltd found in 1990, is located in Jiangbei Industry Zone of Nanjing, Jiangsu Province, which is near the beautiful Yangtze River. Our plant covers an area of 50,000 square meters with the registered capital of RMB 100 million.
Our products mainly involve two series: series of ParaToluenesulfonic Acid and ParaTertButyl Benzoic Acid. Series of 4-Toluene Aulfonic Acid: P-Toluenesulfonic Acid PTSA, P -Toluene Sulfonic Acid 65% water solution, Sodium P-Toluene Sulfonate, Sodium Xylene Sulphonate and its main raw materials.

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